Process of making soap powders.



unrrnu STATES PATENT OFFICE.

CARLETON ELLIS, F LARCHMONT, NEW YORK, ASSIGNOR T0 ELLIS-FOSTER COMPANY,

A CORPORATION OF NEW JERSEY.

PROCESS OF MAKING SOAP POWDERS.

No Drawing.

To all whom it may concern:

Be it known that I, CARLETON ELLIS, a citizen of the United States, residing at Larchmont, in the county of \Vestchester and State of New York, have invented cert-ain new and useful Improvements in Procvfying the grease, or soap esses of Making Soap Powders, of which the following is a specification.

This invention relates to processes of making soap powders or soap material, preferably in a powdered form, and relates particularly to the production of light and fluffy hydrated soap powders having the desirable feature of extreme solubility 111 water.

The present methods of manufacturing soap and soap powders mostly involve the protracted and costly method of saponistock, with alkaline solutions, salting out the soap, crutching and setting in frames, and subsequently slicing, drying, reducing to a granular condition-,redrying and grinding to a powder, or mixing with soda ash, or other detergent or filling material. The manipulation, etc., which these preparations have to undergo makes them relatively dense and insoluble which is disadvantageous since the great advantage to be derived from the use of soap powders over cake soap is the rapidity of their solution in water. ble a soap powder, the more commercially useful it will be found.

My invention involves, the manufacture of soap powders and similar soap material without the use of a large quantity of water for the purpose of saponification, and by a. method which brings about the direct combination of the soap stock and alkali, so as to form a soap product which is light, fluffy and porous and of extreme solubility.

There have been proposed a number of so-called quick processes, which are mostly inoperative, or produce unsatisfactory products, through inability to properly combine the materials under suitable conditions of operation to produce a soluble efficient de- 1 ter gent. I have found that fatty acids produced in the autoclave hydrolysis of greases are particularly susceptible to combination with alkalis under certain conditions, as will be hereinafter described. I have found, however, that the mixed fatty acids, such as are ordinarily produced from the autoclave saponification of common fats, do not Specification of Letters Patent.

Application filed March 13, 1908. Serial No. 420,765.

The more solu-' Patented Oct. 8, 1912.

yield ordinarily a product as satisfactory as does the oleic acid which these fatty acids contain. I prefer, therefore, to press out from this so called still stock, the red oil, or oleic acid, and use this liquid oil, or fat acid material, for treatment in accordance with my process. I have found that the product from red oil has greater detergent property than soaps made from the mixed acids, or from the individual acids, stearic or palmitic acids. The red oil soap products have the additional advantage of not gelatinizing to the same extent when hot solutions of such soaps are cooled. It is probable also that the oleic mixtures made by my process are less hydrolized in solution, so that their causticity is not as pronounced as ordinary soap compositions. My process involves the treatment of such soap stock, preferably red oil, as stated, with an excess of soda ash and with water in such relative proportions that a dry product quickly results from the mixture and in such a manner that the spontaneous heat of reaction between the red oil and the soda ash, as well as the heat of the solution, or hydration, of the soda ash, brings about the complete or substantially complete saponification of the soap stock. This permits of the manufac ture of the product without the use of steam or steam jacketed kettled or heatin apparatus, so that the operation may e conducted, so to speak, in the cold, although the spontaneous rise in temperature, due to the reaction, causes the mass to attain a temperature of 125 to 135 F., more'or less, according to the conditions of operation. This spontaneous heating, which eliminates the necessity of steam jacketed kettles, or the blowing in of steam into the mixture, greatly simplifies the process of manufacturing, reduces the cost of machinery, materially shortens the time of manufacture and furnishes a product which has certain novel qualities, as will be hereinafter described.

By mixing red oil with anhydrous sodium carbonate or soda ash, and subsequently adding a limited quantity of Water,a plastic mass results. The water and oil incorporate together because of the emulsifying power of the alkali and of the soap which forms. The oil and the water cooperate together to form the fluid component of the magma. The dry soda carbonate in taking up this water as it soon does, evolves considerable heat and in turn the oleic acid 1n reacting upon the sodium carbonate evolves still further heat, so that the mass becomes the-reaction, if the proper amount of water has been employed, and after the mass is cooled down to ordinary temperature, it forms a light, fluffy and readily disintegrating body of dry soap. This mass is readily reduced to a fine powder, and the particles of the powder are also fluffy, since they result from breaking down the vesicular mass and are naturally in large part curvilinear. Particles such as these float in water and do not form the hard compact dough which is formedunder similar circumstances by a soap powder consisting of dense, hard particles.

An illustrative formula setting forth my at present regarded preferred embodiment, is made by mixing together in a suitable mixing device, such as a tub, or kettle with revolving stirrers, a charge consisting of 20 lbs. of red oil, 50 lbs. of soda ash and 15 quarts of water, or about a third of the amount of water necessary to completely hydrate the soda ash. The amount of soda ash is considerably larger than that equivalent to the red oil. The red oil is preferably run into the mixer first, this is immediately followed by the soda ash and then the water is quickly added. The mixture forms a pasty mass, the temperature'of which spontaneously rises to about 130 F. and this paste is run from the mixer on to a cooling floor, where it is allowed to remain undisturbed and where it quickly cools and har dens. During the cooling operation. a peculiar phenomenon evinces itself. The mass undergoes a sort of disintegration whereby it becomes extremely friable and spongy, being intimately Vesiculated by the evolved carbon dioxid, and swells in volume. The phenomenon is optically somewhat like that of the slaking of lime, except that in the case of the soap mixture described, the expansion in volume is not nearly as great as that which occurs in the slaking of lime.

The expansion which does occur. however, is

sufficient to break up the hard lumps and particles into fine soft powdery material, which can be reduced to the size of the grains of ordinary soap powder by merely rubbing bet-ween the hands. Hence a very simple grinding machine may be used for reducing it to a powdered form, giving soap grains each of which is intimately porous or vesiculated. This expansive disintegrzr constitutes an mg the spontaneously comminuted or disintegrated product, reduces the time of manufacture and cost of machinery, also the labor involved, to a minimum; which is a very important consideration in view of the great competition prevailing at the present time in the manufacture of such .preparations.

I may, of course, use various other soap stocks with the red oil, or with the other fatty acids mentioned above, and foracheap preparation may add a considerable pro portion of rosin. I have, for instance, made up numerous compositions consisting of red oil and rosin, or still stock and rosin, in

varying proportions. One formula which I find fairly satisfactory for a cheap article, consists of 1 lb. each of red oil and resin, 5 lbs. of soda and 3 pints of water. The rosin should be melted with the red oil before the addition with the soda ash and water.

Various abrasive materials may be added, if desired, such as tripoli, ground pumice stone, silex, or rotten stone, and the like. The.

usual detergent materials such as borax, and the like, talc, etc., may also be introduced.

For certain purposes, where a very caustic product is desired, I make use of caustic soda or caustic potash in small amount in connection with the described substances. Such a mixture may be made by mixing 2 lbs. or so, of red oil, 4:}- lbs. of soda ash and lb. of caustic soda, to which is added about 3 pints of water. Under certain circumstances, I find it possible to add the water through the agency of Washing soda. crystallized sodium carbonate contains some 60% of water, and by grinding the crystals, or crushing them and mixing wit-h the soda ash and red oil, the water may be added in that form, and I find under certain circumstances that this is a useful method of procedure, but it affords the disadvantage of making a rather denser product, which does not heat spontaneously to the same temperature, and which often times requires artificial heat to bring about the desired reaction. The denser product which is produced by this method does not yield as .soluble a soap as the products above men tioned. It is better to add the quantity of Water necessary directly in lieu of using crystallized sodium carbonate to furnish it. I have, however, observed that/when caustic soda is introduced into the soap powder for the purpose of making a caustic preparation for certain purposes, that if the pr0cor fillers such as sodium sulfate,

character, and may ess is conducted by the direct addition of water, that the resulting soap powder is disposed to exhibit slight hydroscopic properties which often times are undesirable. If, however, it is made through the addition of washing soda to supply water for the reaction, the product is of a satisfactory be preserved for a long period of time without becoming damp or lumpy. Crystallized carbonate of soda may he therefore used to some extent in conncc' tion with mixtures containing caustic soda.

Suitable formulae illustrative of these methods of operation comprises, for a noncaustic preparation. 2 lbs. of red oil, 4 lbs. of soda ash and 4 lbs. of carbonate of soda crystals. The caustic preparation may be made by mixing 1 lb. of mixed fatty acids or still stock, 1 lb. of red oil, 4 lbs of soda ash, 1 lb. of caustic soda and 3 lbs. of earbonate of soda crystals. Gentle heating often facilitates the reaction and tends to make a more uniform product where the water is supplied through the agency of the crystallized carbonate of soda. \Vhile it is desirablein this case to crush the crystallized soda so as to pass, say a 20 mesh sieve, I have also operated with a much coarser material, and even with the large crystals themselves.

For textile work it is sometimes desirable to have a considerable proportion of potash present in the soap powder, and a suitable composition containing potash is made by treating in a similar manner 25 parts of potash, 25 parts of soda ash, 20 parts of red oil and 10 parts of still stock to which are added some 10 or 15 parts of water.

Various perfuming agents maybe used in these mixtures, such, for instance, as small percentages of safrol, oil of mirbane, oil of lemon grass, and the like.

The soap composition made with washing soda crystals is better adapted for compression or formation into cakes or chip soap than is that made by the employment of soda ash and water. I find it possible to make solid cakes of attractive appearance containing considerably more saponified matter than is desirable in the use of soap powders. I also find it possible to incorporate abrasive, or fillin material or detergent material, as wel as hydro-carbon bodies, such as naphtha or kerosene. It is also possible to add carbolic acid, pine tar, and the like, or carbonate or sulfate of ammonia, to get a soap having special detergent properties.

Instead of usi g water alone in making soap products above mentioned, I may, of course, use solutions such, for instance, as a solution of silicate of soda. For making soap powder, the process should, however, be preferably conducted along the lines set forth above, that is to say, a predominating amount of soda ash should be mixed with a lesser amount of free fatty acid, preferably red oil, and preferably with water in an amount intermediate the quantity of soap stock and the quantity of soda ash employed, whereby reaction rapidly occurs and a pasty material is produced having by virtue of the spontaneous heating occurring from the soap making process and the heat developed by the hydration of the soda ash, its soap stock completely saponified furnishing a product which on cooling, expansively comminutes or disintegrates to form pulverulent, or partially pulverized, saponaceous material capable of being rapidly and efficiently ground or sifted to the degree of fineness required in commercial soap powders.

While the specific method vof mixing as above set forth is to be recommended the procedure may be varied through the addition of the ingredients in ditferent ways or sequence. Hot water may be used if desired and the addition of the water may be made gradual. It should be observed that the amount of water used is insufiicient to dissolve the alkali employed; whereby hydrated or partially hydrated carbonated alkali results. The partially hydrated carbonated alkali also may be obtained by mixing a nearly anhydrous alkali such as soda ash with a hydrated alkali such as washing soda, with the disadvantage however that with the latter mixture less spontaneous heating occurs.

Having described my invention, to the details of which I, of course, do not wish to be limited, what I claim is 2- 1. The process of making a soap product which comprises mingling a free fatty acid with dry soda ash and water in amount sufficient to institute a reaction while insufiicient for the solution of said soda ash, said mingling being done at ordinary temperatures, allowing the mixture to heat spontaneously until a self-disintegrating product is obtained and to cool undisturbed, and comminuting the product.

2. The process of making a soap product which comprises mingling about 2 parts of red oil, about 5 parts of dry soda ash and about 3 parts of water, said mingling being done at ordinary temperatures, allowing the mixture to heat spontaneously until a selfdisintegrating product is obtained and to cool undisturbed, and comminuting the product.

3. The process of making a son product which comprises mingling a free fatty acid with an alkaline composition capable of developing heat on hydration, mixing with water in amount sutlicient to develop such heat while insufficient to dissolve such alkaline composition, said mixin being done at allowing the ordinary temperatures, an

K mixture to heat spontaneously until a selfdry carbonate of. soda, thereafter adding disintegrating product is obtained and to water in amount insufficient to dissolve such cool undisturbed carbonate; allowing the mixture to heat 4. The process of making a soap product spontaneously until a self-disintegrating 5 which comprises mixing a fatty acid with a product is obtained and allowing the 'mix- 20 dry carbonate of soda, and thereafter adture to cool undisturbed, said addition and mixing water in amount insufficient to disadmixture being performed at ordinary solve such carbonate, allowing the mixture temperatures.

to heat spontaneously until a self-disinte- In testimony whereof I have afiixed my 10 grating product is obtained and allowing signature in presence of two witnesses.

the mixture to cool undisturbed said admixture being performed at ordinary tempera- CARLETON ELLIS tures. Witnesses 5. The process of making a soap product HARRY W. BROWN,

15 which comprises admixing red oil with a BIRDELLA M. ELLIsf 

